WO2013031279A1 - Ｃｕ－Ｎｉ－Ｓｉ系合金及びその製造方法 - Google Patents

Ｃｕ－Ｎｉ－Ｓｉ系合金及びその製造方法 Download PDF

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WO2013031279A1
WO2013031279A1 PCT/JP2012/059207 JP2012059207W WO2013031279A1 WO 2013031279 A1 WO2013031279 A1 WO 2013031279A1 JP 2012059207 W JP2012059207 W JP 2012059207W WO 2013031279 A1 WO2013031279 A1 WO 2013031279A1
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orientation
copper
mass
alloy
cold rolling
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PCT/JP2012/059207
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French (fr)
Japanese (ja)
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真之 長野
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Jx日鉱日石金属株式会社
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Priority to CN201280042580.XA priority Critical patent/CN103781925A/zh
Priority to KR1020147007915A priority patent/KR101628583B1/ko
Publication of WO2013031279A1 publication Critical patent/WO2013031279A1/ja

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    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C9/00—Alloys based on copper
    • C22C9/06—Alloys based on copper with nickel or cobalt as the next major constituent
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22F—CHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
    • C22F1/00—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
    • C22F1/08—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working of copper or alloys based thereon
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
    • H01B1/00—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors
    • H01B1/02—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors mainly consisting of metals or alloys
    • H01B1/026—Alloys based on copper

Definitions

  • the present invention relates to a copper alloy having excellent strength and bending workability, which is suitable as a conductive spring material for connectors, terminals, relays, switches and the like, and a method for producing the same.
  • the copper alloy used for these components is required to have good strength and electrical conductivity.
  • the copper alloy used is required to have good strength and electrical conductivity.
  • in-vehicle female terminals are often subjected to a notching process called notching on the inner surface of the bending before press bending. This is processing performed to improve the shape accuracy after press bending. With the miniaturization of products, notching processing tends to become deeper in order to further improve the shape accuracy of terminals. Therefore, a copper alloy used for a vehicle-mounted female terminal is required to have good bending workability in addition to good strength and electrical conductivity. Further, as the relay terminal is miniaturized, the material is required to have good bending workability because the material is subjected to tight bending to obtain a desired strength.
  • precipitation strengthened copper alloys such as a Corson alloy having high strength and electrical conductivity are used, and the demand is increasing.
  • Corson alloys Cu-Ni-Si alloys have both high strength and relatively high electrical conductivity.
  • the strengthening mechanism is based on the precipitation of Ni-Si intermetallic particles in the Cu matrix.
  • the conductivity is improved.
  • strength and bending workability are contradictory properties, and it is desired to improve bending workability while maintaining high strength even in Cu—Ni—Si based alloys.
  • Patent Document 1 As a method for improving the bending workability of the Cu—Ni—Si alloy, there is a method of controlling the crystal orientation as described in Patent Documents 1 to 3.
  • the area ratio of ⁇ 001 ⁇ ⁇ 100> in the measurement result of EBSD analysis is set to 50% or more.
  • Patent Document 2 the area ratio of ⁇ 001 ⁇ ⁇ 100> in the measurement result of EBSP analysis is 50%.
  • the area ratio of ⁇ 110 ⁇ ⁇ 112> in the measurement result of EBSD analysis is 20% or less, and the area ratio of ⁇ 121 ⁇ ⁇ 111> is 20%.
  • the bendability is improved by setting the area ratio of ⁇ 001 ⁇ ⁇ 100> to 5 to 60%.
  • Patent Document 4 bending workability is improved by setting the work hardening index to 0.05 or more.
  • the present inventors conducted a verification test on the effect of the preceding invention.
  • a certain improvement effect was recognized, but the bending radius was 0.
  • the present invention provides a Cu—Ni—Si alloy having excellent strength and bending workability, which is suitable as a conductive spring material for connectors, terminals, relays, switches and the like, and a method for producing the same.
  • the conventional technology improves the bending workability of Cu-Ni-Si alloys by controlling the crystal orientation of the copper alloy, but not only controls the crystal orientation but also controls the work hardening index (n value). As a result, it was found that excellent bending workability can be obtained.
  • the present invention completed on the basis of the above knowledge, in one aspect, contains 1.0 to 4.5 mass% Ni and 0.2 to 1.0 mass% Si, with the balance being copper and inevitable impurities.
  • EBSD Electron Back-Scatter Diffraction: Electron Backscattering Diffraction
  • the area ratio of the Cube orientation ⁇ 0 0 1 ⁇ ⁇ 1 0 0> is 5% or more
  • the Brass orientation The area ratio of ⁇ 1 ⁇ 1 0 ⁇ ⁇ 1 1 ⁇ 2> is 20% or less
  • the area ratio of Copper orientation ⁇ 1 1 2 ⁇ ⁇ 1 1 1> is 20% or less
  • the work hardening index is 0.2 or less.
  • the Cu—Ni—Si based alloy according to the present invention includes at least one of Sn, Zn, Mg, Fe, Ti, Zr, Cr, Al, P, Mn, Co, Cr and Ag in a total amount. 0.005 to 2.5 mass% is contained.
  • an ingot containing 1.0 to 4.5 mass% Ni and 0.2 to 1.0 mass% Si, the balance being copper and inevitable impurities is produced.
  • the ingot is hot-rolled, cold-rolled, heat-treated with a softening degree of 0.25 to 0.75, then cold-rolled with a working degree of 7 to 50%, and then solutionized.
  • This is a method for producing a Cu—Ni—Si based alloy of the present invention, in which after the treatment, aging treatment and cold rolling at a strain rate of 1 ⁇ 10 ⁇ 4 (1 / second) or less are performed in an arbitrary order.
  • the ingot is made of Sn, Zn, Mg, Fe, Ti, Zr, Cr, Al, P, Mn, Co, Cr, and Ag. One or more of them are contained in a total amount of 0.005 to 2.5% by mass.
  • the present invention is a copper-drawn product provided with the above copper alloy.
  • the present invention is an electronic device component including the copper alloy.
  • FIG. 4 is a graph showing the relationship between the annealing temperature and the tensile strength when the Cu—Ni—Si based alloy according to the present invention is annealed at various temperatures.
  • Ni and Si concentration Ni and Si are precipitated as an intermetallic compound such as Ni 2 Si by aging treatment. This compound improves the strength, and by precipitation, Ni and Si dissolved in the Cu matrix are reduced, so that the conductivity is improved.
  • the Ni concentration is less than 1.0% by mass or the Si concentration is less than 0.2% by mass, the desired strength cannot be obtained, and conversely, when the Ni concentration exceeds 4.5% by mass or the Si concentration is 1.
  • the Ni concentration is controlled to 1.0 to 4.5 mass% and the Si concentration is controlled to 0.2 to 1.0 mass%.
  • the Ni concentration is preferably 1.3 to 4.0% by mass
  • the Si concentration is preferably 0.3 to 0.9% by mass.
  • the Cu—Ni—Si based alloy according to the present invention preferably contains these elements in a total amount of 0.005 to 2.5% by mass, and preferably 0.1 to 2.0% by mass. More preferred.
  • the Cube orientation is a state in which the (0 0 1) plane is oriented in the rolling surface normal direction (ND) and the (1 0 0) plane is oriented in the rolling direction (RD), and ⁇ 0 0 1 ⁇ It is indicated by an index of ⁇ 1 0 0>.
  • the Brass orientation is a state in which the ND faces the (1 1 0) plane and the RD faces the (1 1 2) plane, and is indicated by an index of ⁇ 1 1 0 ⁇ ⁇ 1 1 2>.
  • the Copper orientation is a state in which the ND faces the (1 1 2) plane and the RD faces the (1 1 1) plane, and is represented by an index of ⁇ 1 1 2 ⁇ ⁇ 1 1 1>.
  • the area ratio of the Cube orientation is controlled to 5% or more. When the area ratio of the Cube orientation is less than 5%, the bending workability deteriorates rapidly.
  • the upper limit of the area ratio of the Cube orientation is not restricted in terms of bendability, but in the case of the Cu—Ni—Si based alloy according to the present invention, the area ratio of the Cube orientation is not affected by any change in the manufacturing method. None exceed 80%.
  • the area ratios of the Copper orientation and the Brass orientation are each controlled to 20% or less. If either the Copper azimuth area ratio or the Brass azimuth area ratio exceeds 20%, the bending workability deteriorates rapidly.
  • the lower limits of the area ratio of the Copper orientation and the Brass orientation are not restricted in terms of bendability, but in the case of the Cu—Ni—Si based alloy according to the present invention, no matter how the production method is changed, the Copper orientation Either the area ratio or the area ratio of the Brass orientation is never less than 1%.
  • n value is a value used as an index of this work hardening. A larger n value indicates that the metal has a greater increase in tensile strength due to work hardening.
  • press bending In order to mold the material into an electronic component such as a connector, press bending must be performed. When press bending is performed, the material is work-hardened and its tensile strength increases. Generally, the tensile strength and bending workability of a material are in a trade-off relationship, and the higher the tensile strength, the worse the bending workability.
  • the n value is controlled to 0.2 or less. n value becomes like this. Preferably it is 0.1 or less, More preferably, it is less than 0.05. When the n value exceeds 0.2, the bending workability deteriorates rapidly.
  • the lower limit of the n value is not restricted in terms of bendability, but in the case of the Cu—Ni—Si alloy according to the present invention, the n value is less than 0.01 no matter how the manufacturing method is changed. There is nothing.
  • strain relief annealing may be performed after the third cold rolling in order to recover the decrease in the spring limit value due to the third cold rolling.
  • pre-annealing heat treatment
  • second cold rolling with a relatively low workability are performed before the solution treatment.
  • the preliminary annealing is performed under the condition that the softening degree S is 0.25 to 0.75.
  • FIG. 1 illustrates the relationship between the annealing temperature and the tensile strength when the Cu—Ni—Si alloy according to the present invention is annealed at various temperatures.
  • thermocouple A sample with a thermocouple attached is placed in a furnace heated to a specified temperature, and when the sample temperature measured by the thermocouple reaches the specified temperature, the sample is removed from the furnace and cooled with water, and the tensile strength is measured. It is a thing. Recrystallization progresses when the sample arrival temperature is 500 to 700 ° C., and the tensile strength is rapidly reduced. The gradual decrease in tensile strength on the high temperature side is due to the growth of recrystallized grains.
  • the softening degree S in the pre-annealing is defined by the following equation.
  • ⁇ 0 is the tensile strength before pre-annealing
  • ⁇ and ⁇ 900 are the tensile strength after pre-annealing and after annealing at 900 ° C., respectively.
  • the temperature of 900 ° C. is adopted as a reference temperature for knowing the tensile strength after recrystallization because the Cu—Ni—Si alloy according to the present invention is stably recrystallized when annealed at 900 ° C. Yes.
  • S is less than 0.25, the area ratio of the Copper orientation increases to exceed 20%, and accordingly, the area ratio of the Cube orientation also decreases.
  • the temperature, time and cooling rate of the pre-annealing are not particularly limited, and it is important to adjust S to the above range. Generally, when a continuous annealing furnace is used, the furnace temperature ranges from 400 to 700 ° C. for 5 seconds to 10 minutes, and when a batch annealing furnace is used, the furnace temperature ranges from 350 to 600 ° C. for 30 minutes to 20 hours. Done in The softening degree S can be adjusted to 0.25 to 0.75 by the following procedure. (1) Measure the tensile test strength ( ⁇ 0 ) of the material before pre-annealing.
  • the material before preliminary annealing is annealed at 900 ° C. Specifically, the material to which the thermocouple is attached is inserted into a tubular furnace at 950 ° C., and when the sample temperature measured by the thermocouple reaches 900 ° C., the sample is taken out of the furnace and cooled with water. (3) Obtain the tensile strength ( ⁇ 900 ) of the material after annealing at 900 ° C. (4) For example, when ⁇ 0 is 800 MPa and ⁇ 900 is 300 MPa, the tensile strengths corresponding to the softening degrees of 0.25 and 0.75 are 675 MPa and 425 MPa, respectively.
  • the annealing conditions are determined so that the tensile strength after annealing is 425 to 675 MPa.
  • “when the sample temperature measured by the thermocouple reaches 900 ° C., the sample is taken out of the furnace and water-cooled” is specifically, for example, the sample is wired in the furnace. When suspended, the wire is cut when it reaches 900 ° C. and dropped into a water tank provided below, or immediately after the sample temperature reaches 900 ° C. by hand from inside the furnace. Take it out quickly by immersing it in a water tank.
  • the strain rate of the present invention is specified as rolling speed / roll contact arc length, and in order to lower the strain rate, it is effective to slow the rolling speed, increase the number of rolling passes, and lengthen the roll contact arc length. Is.
  • the lower limit of the strain rate is not limited from the point of the n value, but if rolling is performed below 1 ⁇ 10 ⁇ 5 (1 / second), the rolling time is long, which is not industrially preferable.
  • the strain rate of rolling in a general industry is about 2 ⁇ 10 ⁇ 4 to 5 ⁇ 10 ⁇ 4 (1 / second).
  • the working degree of cold rolling (3) is preferably 30 to 99%. In order to generate recrystallized grains partially by pre-annealing (4), it is necessary to introduce strain by cold rolling (3), and effective strain can be obtained at a workability of 30% or more.
  • Cold rolling (7) and (9) is arbitrarily performed for increasing the strength and controlling the n value, and the strength increases with an increase in the rolling degree, but the bendability decreases.
  • the effects of the present invention can be obtained regardless of the degree of cold rolling (7) and (9).
  • the strain relief annealing (10) is optionally performed in order to recover the spring limit value and the like which are lowered by the cold rolling when the cold rolling (9) is performed.
  • the effect of the present invention can be obtained regardless of the presence or absence of strain relief annealing (10).
  • the strain relief annealing (10) may or may not be performed.
  • general production conditions for the Cu—Ni—Si based alloy may be selected.
  • the Cu—Ni—Si based alloy according to the present invention can be processed into various copper products, such as plates, strips and foils. Furthermore, the Cu—Ni—Si based alloy according to the present invention can be used for lead frames and connectors. It can be used for electronic parts such as pins, terminals, relays, switches, and foil materials for secondary batteries. Further, the final plate thickness (product plate thickness) of the Cu—Ni—Si alloy according to the present invention is not particularly limited, but is generally 0.05 to 1.0 mm in the case of the above product use.
  • Example 1 An alloy containing Ni: 2.6% by mass, Si: 0.58% by mass, Sn: 0.5% by mass, and Zn: 0.4% by mass with the balance being copper and inevitable impurities is used as an experimental material. , Pre-annealing, workability of the second cold rolling and the relationship between the strain rate of the third cold rolling and the crystal orientation and n value, and the influence of the crystal orientation and n value on the bendability of the product .
  • a high-frequency melting furnace 2.5 kg of electrolytic copper was melted using a graphite crucible having an inner diameter of 60 mm and a depth of 200 mm in an argon atmosphere.
  • Pre-annealing Insert a sample into an electric furnace adjusted to a predetermined temperature and hold it for a predetermined time, then place the sample in a water bath for cooling (water cooling), or leave the sample in the atmosphere for cooling (air cooling) 2 Cooled under street conditions.
  • Second cold rolling Cold rolling was performed at various rolling degrees to a thickness of 0.18 mm.
  • Solution treatment The sample was inserted into an electric furnace adjusted to 800 ° C. and held for 10 seconds, and then the sample was placed in a water bath and cooled.
  • Aging treatment Heated in an Ar atmosphere at 450 ° C. for 5 hours using an electric furnace.
  • a common rotation axis that can be expressed at the smallest angle is adopted.
  • the deviation angle is calculated for all measurement points, and the first decimal place is an effective number.
  • the area of crystal grains having an orientation within 10 ° from each of the Cube orientation, Copper orientation, and Brass orientation is the total measurement area. To obtain the area ratio.
  • the information obtained in the azimuth analysis by EBSD includes azimuth information up to a depth of several tens of nanometers in which the electron beam penetrates the sample, but is described as an area ratio because it is sufficiently small with respect to the measured width. .
  • Table 1 shows test conditions and evaluation results.
  • the inventive examples were produced under the conditions specified by the present invention, the crystal orientation and the n value satisfied the specifications of the present invention, and MBR / t was 0.5 or less and good bending workability was obtained.
  • Comparative Example 1 since the degree of softening in the pre-annealing was less than 0.25, the area ratio of Copper orientation exceeded 20%, and the area ratio of Cube orientation was less than 5%.
  • Comparative Example 2 since the degree of softening in the preliminary annealing exceeded 0.75, the area ratio of the Brass orientation exceeded 20%, and the area ratio of the Cube orientation became less than 5%.
  • Comparative Examples 3 and 4 the degree of workability of the second rolling deviated from the definition of the present invention, and the area ratio of the Cube orientation was less than 5%.
  • Comparative Example 5 the strain rate of the third rolling deviated from the definition of the present invention, and the n value exceeded 0.2.
  • MBR / t was 1, and bending workability was poor. Note that Comparative Example 5 was performed within the range of conditions recommended by Patent Document 3, and the crystal orientation satisfied the provisions of Patent Document 2.
  • Example 2 It was examined whether the bendability improving effect shown in Example 1 could be obtained with Cu—Ni—Si based alloys having different components and production conditions. Casting, hot rolling and surface grinding were performed in the same manner as in Example 1 to obtain a 9 mm thick plate having the components shown in Table 2. The plate was subjected to rolling and heat treatment in the following process order to produce a product sample having a plate thickness of 0.15 mm.
  • First cold rolling Cold rolling was performed to a predetermined thickness in accordance with the rolling degree of the second cold rolling.
  • Pre-annealing Insert a sample into an electric furnace adjusted to a predetermined temperature and hold it for a predetermined time, then place the sample in a water bath for cooling (water cooling), or leave the sample in the atmosphere for cooling (air cooling) Cooling was performed under two conditions.
  • Second cold rolling Cold rolling was performed at various rolling degrees to a thickness of 0.18 mm.
  • Solution treatment The sample was inserted into an electric furnace adjusted to a predetermined temperature and held for 10 seconds, and then the sample was placed in a water bath and cooled. The temperature was selected so that the average diameter of the recrystallized grains was in the range of 5 to 25 ⁇ m.
  • Aging treatment Heating was performed in an Ar atmosphere using an electric furnace at a predetermined temperature for 5 hours.
  • the temperature was selected to maximize the tensile strength after aging.
  • Third cold rolling Cold rolling was performed at various strain rates from 0.18 mm to 0.15 mm at a working degree of 17%.
  • Strain relief annealing The sample was inserted into an electric furnace adjusted to a predetermined temperature and held for 10 seconds, and then the sample was left in the air and cooled.
  • Example 2 Evaluation similar to Example 1 was performed about the sample after pre-annealing, and a product sample.
  • Tables 2 and 3 show test conditions and evaluation results, respectively.
  • “none” is written in the temperature column.
  • the alloy of the present invention contains Ni and Si at the concentrations specified by the present invention, and is manufactured under the conditions specified by the present invention.
  • the crystal orientation and the n value satisfy the specifications of the present invention, and MBR / t is 0. Bending workability as good as .5 or less was obtained.
  • Comparative Example 6 since the strain rate of the third rolling deviated from the definition of the present invention, the n value exceeded 0.2 and the bending workability was poor.
  • Comparative Examples 7, 8 and 9 the degree of softening in the pre-annealing was out of the definition of the present invention, and in Comparative Examples 10 and 11, the degree of work in the second rolling was out of the definition of the present invention. Beyond the provisions of the invention, the bending workability was poor. In Comparative Example 12, the Ni and Si concentrations were lower than those of the present invention, and the bending workability was good, but the 0.2% proof stress did not reach 500 MPa.

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PCT/JP2012/059207 2011-08-29 2012-04-04 Ｃｕ－Ｎｉ－Ｓｉ系合金及びその製造方法 WO2013031279A1 (ja)

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CN201280042580.XA CN103781925A (zh) 2011-08-29 2012-04-04 Cu-Ni-Si系合金及其制造方法
KR1020147007915A KR101628583B1 (ko) 2011-08-29 2012-04-04 Cu－Ni－Si 계 합금 및 그 제조 방법

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JP2011-185962 2011-08-29
JP2011185962A JP5117604B1 (ja) 2011-08-29 2011-08-29 Ｃｕ−Ｎｉ−Ｓｉ系合金及びその製造方法

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CN103509970A (zh) * 2013-08-16 2014-01-15 中国船舶重工集团公司第七二五研究所 一种铜镍铝硅弹性合金及其制备方法
JP6310538B1 (ja) * 2016-12-14 2018-04-11 古河電気工業株式会社 銅合金線棒材およびその製造方法

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CN109072341B (zh) * 2016-03-31 2021-07-27 同和金属技术有限公司 Cu-Ni-Si系铜合金板材和制造法
CN106591623B (zh) * 2016-12-05 2018-04-17 宁波博威合金板带有限公司 一种耐高温铁青铜及其制备方法和应用
JP6609590B2 (ja) * 2017-03-30 2019-11-20 Ｊｘ金属株式会社 層状組織を有する高強度チタン銅条および箔
JP6609589B2 (ja) * 2017-03-30 2019-11-20 Ｊｘ金属株式会社 層状組織を有する高強度チタン銅条および箔
JP6378819B1 (ja) * 2017-04-04 2018-08-22 Ｄｏｗａメタルテック株式会社 Ｃｕ−Ｃｏ−Ｓｉ系銅合金板材および製造方法並びにその板材を用いた部品
CN107326215A (zh) * 2017-08-15 2017-11-07 徐高杰 一种槽楔用铜合金的加工方法
JP6670277B2 (ja) * 2017-09-14 2020-03-18 Ｊｘ金属株式会社 金型摩耗性に優れたＣｕ−Ｎｉ−Ｓｉ系銅合金
CN111485132B (zh) * 2020-04-10 2021-09-10 宁波博威合金板带有限公司 一种综合性能优异的铜合金带材及其制备方法

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